Our invention relates to olfactorily active component-containing microparticles which are useful in augmenting, enhancing and/or imparting aroma and/or taste (over relatively long periods of time in a controllably releasable manner) to perfume compositions, perfumed articles, foodstuffs, chewing gums, beverages and the like.
A particular need exists for deodorant and antiperspirant compositions having pleasant fragrances which last for a relatively long period of time on use. Furthermore, a particular need exists for chewing gums, for example, having a pleasant flavor which lasts for a relatively long period of time.
It is known in the prior art to produce compositions for contacting the skin wherein a fragrance is released from the composition after application of the composition to the skin, that is, body activated fragrances. It is desired that such products produce a low level of odor prior to application to the skin, but which release fragrance over a long period of time after application to the skin.
It is also known in the art to control human body odors by use of deodorant products, particularly in the underarm area of the body. Deodorant products generally contain a perfume or other odor masking ingredients in a vehicle from which active ingredients may be deposited on the skin. The deodorant products may be in the form of solid or semisolid sticks.
Furthermore, it is known to delay release of the fragrance from a composition by methods such as microencapsulation of the fragrance substance. By the same token, it is known to delay release of flavors from the composition by methods such as microencapsulation of the flavor substance.
However, a delayed fragrance release from a deodorant stick has not effectively been obtained using microencapsulation principally because microencapsulating a fragrance in a water-containing deodorant stick base dissolves the protective microencapsulation coating and prematurely releases the fragrance. Indeed, several attempts at attaning fragrance longevity for such antiperspirant and deodorant products have been made in the art employing encapsulation and spray drying techniques. Prior methods have produced inconsistent results, either because they have involved a rupturing of microcapsule walls by mechanical pressure to achieve fragrance release or encapsulating polymers have generally presented incompatibility problems with the fragrance resulting in distortion of the fragrance profile.
By the same token, a delayed flavor evolution from a chewing gum stick has not been effectively obtained using microencapsulation, principally because microencapsulating a flavor in a chewing gum stick activated by water dissolves the protective microencapsulation coating and prematurely releases the flavor, so that after several minutes of chewing, no flavor remains. Indeed, several attempts at attaining flavor longevity for such chewing gum products and the like have been made in the art employing encapsulation and spray drying techniques. Prior methods have produced inconsistent results, either because they have involved a rupturing of microcapsule walls by mechanical pressure to achieve flavor release or encapsulating polymers have generally presented incompatibility problems with the flavor resulting in distortion of the flavor profile.
U.S. Pat. No. 5,614,179 teaches deodorant products containing a polymer/fragrance encapsulated by carbon and ingredient A deodorant or antiperspirant-deodorant cosmetic stick comprises an organic matrix having a dispersed particle phase of an encapsulated bicarbonate salt such as sodium bicarbonate. The particle surfaces are coated with a film forming medium comprising a blend of a polymer and a fragrance. When this product is applied to underarm surfaces, the deodorizing activity is signaled by the release of a fragrance aroma.
U.S. Pat. No. 4,731,243, which is incorporated herein by reference, teaches deodorant and/or antiperspirant sticks which contain suspended therein fragrance containing polymeric pellets containing 1 to 80% fragrance. The polymeric pellets are produced by means of cryogenically grinding an extruded mixture of perfume composition and polymer. U.S. Pat. No. 4,428,869, which is also incorporated herein by reference, teaches a microcapsule suspension of a fragrance which yields a continuously high fragrance intensity release, evenly and uniformly over an extended period of time. None of these prior disclosures achieve a fragrance release evenly over a long period of time resulting from contact with skin moisture.
Accordingly, it is still desired to provide deodorant or antiperspirant compositions having a delayed release of fragrance evenly over an extended period of time. It is particularly desired to provide such product wherein the fragrance is released after contact of the composition with skin moisture.
With respect to encapsulated flavors, U.S. Pat. No. 5,603,971 issued on Feb. 18, 1997 and U.S. Pat. No. 5,897,897 issued on Apr. 27, 1999, each disclose a flavor encapsulation composition comprising:
(a) a flavoring material encapsulated in;
(b) a glassy matrix of matrix components consisting essentially of 85 to 95 weight percent of a modified starch and 5 to 15 weight percent of a polyhydric alcohol wherein said polyhydric alcohol is selected from the group consisting of propylene glycol and glycerin and wherein the composition is prepared by a process comprising:
(i) mixing (a) said modified starch; (b) a component selected from the group consisting of polyhydric alcohol and mixtures of polyhydric alcohol with water; and (c) a flavor composition in an extruder to obtain a melted matrix; and
(ii) extruding the melted matrix.
Among the flavoring agents disclosed in U.S. Pat. No. 5,897,897 and in U.S. Pat. No. 5,603,971 are natural extracts, oleoresins, essential oils, protein hydrolysates, aqueous reaction flavors and compounded flavors.
U.S. Pat. No. 3,314,803 issued on Apr. 18, 1967 entitled xe2x80x9cMANNITOL FIXED FLAVOR AND METHOD OF MAKING SAMExe2x80x9d discloses a process for making a dry flavor enhancer containing a stable level of acetaldehyde in an amount effective to produce flavor enhancement, which comprises forming an aqueous solution of mannitol and acetaldehyde and spray drying said solution to obtain a powder product More specifically, U.S. Pat. No. 3,314,803 discloses a process for making a dry, stable flavor enhancer containing acetaldehyde in an amount effective to produce flavor enhancement up to about 4% by weight, which comprises forming a supersaturated solution of 2-10 parts by weight of mannitol and 1-2 parts by weight of acetaldehyde in parts by weight of water; cooling said solution to below about room temperature without crystallizing the mannitol; atomizing said solution into droplets; and passing said droplets through a drying chamber whereby a powdered product is obtained.
Nothing in any of the foregoing references discloses techniques for the production of the microparticles of our invention or processes for producing same, with said microparticles having unexpected, unobvious and advantageous properties with respect to the controllable release of olfactorily active components contained in a matrix in said microparticles.
Our invention is directed to a particulate composition comprising microparticles which are capable of controllably releasing olfactorily active substances, each of which microparticle has an effective diameter of from about 10 up to about 50 microns, and each of which microparticle has a matrix of flavor composition-bearing, flavor component-bearing, perfume composition-bearing or perfume component-bearing silica particles intimately admixed with a saccharide composition consisting essentially of a mixture of maltose and mannitol.
Our invention is further directed to a process for preparing such microparticles, which controllably release one or more aroma chemicals, perfume compositions, flavor compositions or flavor components therefrom into the environment surrounding said particles, comprising the steps of:
(a) adsorbing a fragrance composition or an aroma chemical composition or a flavor composition or a flavor component onto silica powder by means of fluidized bed plating in order to provide a flavor composition-bearing, a perfume composition-bearing, a perfume component-bearing or a flavor component-bearing silica powder composition;
(b) providing a molten saccharide composition consisting essentially of a mixture of maltose and mannitol;
(c) providing an extruder having an extruder input zone and an extruder output zone and having a screw speed of 150-400 rpm;
(d) substantially simultaneously introducing (i) said saccharide composition and (ii) said flavor composition-bearing, said fragrance composition-bearing, said fragrance component-bearing or said flavor component-bearing silica composition into the extruder at the extruder input zone;
(e) effecting the blending for a residence time of 30-150 seconds at a temperature in the range of from about 90xc2x0 C. up to about 140xc2x0 C. of the saccharide composition with the flavor composition-bearing, fragrance composition-bearing, flavor component-bearing or fragrance component-bearing silica powder composition in the extruder on operation of the extruder, whereby a fragrance composition-bearing, fragrance component-bearing, flavor composition-bearing or flavor component-bearing silica-saccharide tow is formed in the extruder and exits from the extruder at the extruder output zone;
(f) causing the resulting tow to solidify using drum chilling; and
(g) converting the resulting solidified drum-chilled tow into particles by means of the unit operation of grinding.
The resulting microparticles are useful in augmenting, enhancing and/or imparting aroma and/or taste (over relatively long periods of time in a controllably releasable manner) to perfume compositions, perfumed articles (e.g., deodorant sticks and antiperspirant sticks), food stuffs, chewing gums, beverages and the like. The microparticles produced according to our invention are particularly useful in augmenting, enhancing and/or imparting aroma and/or taste over relatively long periods of time in a controllably releasable manner to deodorant sticks, antiperspirant sticks and chewing gum.
More specifically, the maltose:mannitol blends used to produce the microparticles of our invention contain a weight ratio of maltose:mannitol of from about 10 parts mannitol:60 parts maltose down to 60 parts mannitol:10 parts maltose. In carrying out the process of our invention, a fragrance or a flavor is first adsorbed onto silica by means of xe2x80x9cplatingxe2x80x9d using a fluidized bed plating apparatus, e.g., a NIRO AEROMATIC(copyright) fluidized bed plating apparatus. Fragrance loadings of between about 40% up to about 70% result in a dry, free flowing, pourable product. Prior to compounding the fragrance-silica resulting from the plating step with the maltose:mannitol product, the mixture of maltose and mannitol is melted, and the resulting maltose:mannitol melt is compounded with the fragrance xe2x80x9cplatedxe2x80x9d silica in an extruder by applied heat and shear.
Any single screw or twin screw extruder may be used, but preferred, is the Werner and Phleiderer extruder.
The extrusion process for carrying out the process of our invention is based on control of two specific variables:
(i) the barrel temperature of the extruder; and
(ii) the flow rate of material being processed through the extruder.
Thus, the range of extruder temperatures in the various barrel zones are from about 80xc2x0 C. up to about 140xc2x0 C.; the screw frequency is from about 150 rpm up to about 400 rpm; the flow rate is from about 8 up to about 20 kg per hour; the barrel pressure may vary from about 10 psig up to about 40 psig; and the average residence time of product being processed within the extruder is from about 30 seconds up to about 150 seconds.
The extrusion tow evolving from the extruder is cooled and particularized via, for example, cryogenic grinding. The cooling step ahead of the grinding step is carried out using a drum chilling unit operation according to standard drum chilling procedure well known to those having ordinary skill in the art. Thus, during the drum chilling procedure, the hot extrudate is forced between two chilled rollers to form flakes. The cooling process lasts for approximately 1-3 minutes for flakes to reach room temperature, and this results in a cooling rate of between about 40 up to about 60xc2x0 C. per minute.
Preferably, the extruder is divided into six different temperature controlled barrel zones between 80xc2x0 C. and 140xc2x0 C.
Subsequent to the drum chilling/cooling process, the resulting product is then subjected to cryogenic grinding using liquid nitrogen as specifically set forth in U.S. Pat. No. 4,731,243, the specification for which is incorporated by reference herein.
The resulting product is then incorporated into materials which require extended release control release flavors, e.g., chewing gum, or extended release control release fragrances, e.g., deodorant or antiperspirant sticks, in accordance with the procedures and examples of, for example, U.S. Pat. No. 4,731,243, the specification for which is incorporated by reference herein.
It is to be emphasized that our invention is also directed to a process for preparing solid particles, which not only controllably release one or more perfume component compositions or perfume compositions or flavor compositions or flavor component compositions (also called xe2x80x9colfactory sense effecting compositions of matterxe2x80x9d), but which also have an initial burst release and a response whereby the olfactory sense effecting compositions of matter are initially released in a relatively fast manner when exposed to water.